US6621039B2 - Method and apparatus for creating a free-form three-dimensional metal part using high-temperature direct laser melting - Google Patents
Method and apparatus for creating a free-form three-dimensional metal part using high-temperature direct laser melting Download PDFInfo
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- US6621039B2 US6621039B2 US09/993,720 US99372001A US6621039B2 US 6621039 B2 US6621039 B2 US 6621039B2 US 99372001 A US99372001 A US 99372001A US 6621039 B2 US6621039 B2 US 6621039B2
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Images
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Definitions
- the present invention relates generally to a method and apparatus for directly sintering metal powder, and more particularly to a method and apparatus for directly sintering metal powder on a work-space platform under a high temperature environment in a layer by layer manner.
- the present invention relates to a method and apparatus that is capable of producing composite parts with two types of material.
- RP technology has been successfully used to provide all kinds of prototypes, such as visual, functional, and production prototypes.
- RP techniques have limited impact if used solely for direct fabrication of prototypes.
- the advantages of RP such as flexibility in free-form fabrication without geometric constraints, fast material processing time, and innovative joining techniques, have great potential in reducing time to fabricate a complex tooling.
- RP techniques are applied on rapid tooling (RT) to shorten the lead-time of tooling preparation and to further reduce the time-to-market of a new product.
- RT rapid tooling
- RT technology is typically categorized as either indirect rapid tooling or direct rapid tooling.
- Indirect rapid tooling processes start with a pattern made by the RP process, and a tooling is duplicated with the pattern by casting or spraying, etc.
- direct tooling processes a tooling is fabricated by the RP machine through sintering, bonding, curing, depositing, etc. without any intermediate steps.
- SLS selective laser sintering
- DMLS direct metal laser sintering
- LG laser generating
- LENS laser engineered net shaping
- the SLS process has been developed by DTM Corporation of Austin.
- the system includes a 50W, CO 2 laser unit, a feed-powder cartridge, a laser scanning unit, a build-cylinder, and a powder feeder.
- a motor drives the powder feeder to a specified amount at which a volume of powder extends above a leveling plane.
- the feed-powder cartridge travels across the leveling plane and delivers the powder to the target area.
- a laser beam is generated by laser apparatus and is deflected by galvanometer-controlled mirrors.
- the rotation of the mirror is controlled by a computer corresponding to the cross-section of the layer of the part to be produced.
- the powder will be selectively fused. Once a layer is finished, the process is repeated until the part is built up, layer by layer.
- Rapid Steel 2.0 is a polymer-coated stainless steel powder. It can be used to create tooling for the bridge or pre-production injection molding. A binder melted during laser sintering holds the stainless steel powder together. In a Rapid Steel process, only polymer-binder is melted. The metal does not melt by the laser during the sintering because the laser energy, e.g., 50W, is not high enough to heat the powder up to the melting point of the metal.
- the insert is prepared for the first furnace cycle, as the mold insert created is now a green part.
- the binder decomposes and the steel powder sinters to form small necks (or bridges) between particles.
- the resulting part which is 60% dense, is called a “brown” insert and is much more durable than the green insert.
- the brown part is placed in a crucible and a measured amount of bronze is placed next to the part.
- the crucible is then placed in the furnace for the second furnace cycle.
- the bronze melts and wicks into the brown part by capillary action, forming the infiltrated part.
- the resulting mold inserts are therefore fully dense.
- the post-process procedure is extremely time consuming and involves considerable effort.
- DTM introduced Copper Polyamide (PA), a heat resistant, thermally conductive composite of copper and plastic that can be used to create tooling for short runs of production equivalent plastic parts.
- PA Copper Polyamide
- the metal powder of copper does not melt. Instead, the plastic composite fuses to bond the powder together.
- DMLS is another metal laser forming process developed by Electro Optics Systems (EOS) of Kunststoff in Germany.
- EOSINT M machine has been developed and commercialized since 1995.
- the machine consists of a 200 W, CO 2 laser unit, a laser scanning unit, a building platform, and a scraper assembly.
- the building process is similar to an SLS process.
- An exemplary method and apparatus are further described in U.S. Pat. No. 6,042,774, issued in Mar. 28, 2000 to Wilkening et al, the entirety of which is herein incorporated by reference.
- a metal powder often used in EOSINT is a mixture of bronze, nickel, and copper-phosphide.
- copper-phosphide melts at 660° C. and acts as the low temperature-binding agent.
- bronze and nickel powders homogenize at high temperature.
- Copper-phosphide powder melts, and the liquid phase penetrates the surrounding cavities, wets the bronze/nickel particles and bonds the particles together. After sintering, the part density is about 70% of the theoretical density of the material.
- LG laser generating
- a six-axis robot programmed to go through the motions necessary to build a particular part.
- the powder metal is fed through a cable to the articulated arm of the robot.
- a laser beam travels through a fiber optic cable to deliver energy.
- LG is the only RT technique able to directly produce filly dense parts (N. P. Karapatis et al. 1998).
- the required laser power and beam quality are usually high, e.g. the laser power is normally higher than 1 kW.
- the process itself induces high thermal stresses that can lead to part failure.
- Geometric accuracy and part stability are difficult to generate because of the lack of supporting material.
- Geometry of the parts is often limited to rather simple shapes. Due to applying high power and laser quality, as well as complicated mechanical structure for powder and laser delivery, the LENS system is more expensive than an SLS system (R. Irving, 1999).
- the present invention overcomes the shortcomings associated with the background art and achieves other advantages not realized by the background art.
- An object of the present invention is to improve production efficiency and product density during the production of three dimensional, layered products.
- An object of the present invention is to provide controlled, reliable part production of components from more than one material and within a high production temperature environment.
- a method for producing a desired, three dimensional metallic part comprising the steps of heating a part production apparatus to a setting temperature; maintaining the setting temperature during a fabrication period; depositing a powder onto a target surface, the powder comprising first and second materials; accurately controlling a layer thickness; preventing the powder from leaking from a primary powder container under a high temperature environment; and sintering a selected portion of the powder corresponding to a relative cross-sectional region of the desired part.
- a sintering apparatus for producing a three dimensional metallic part from at least one metallic powder
- the sintering apparatus comprising a laser for selectively melting the at least one metallic powder; a scanner head mounted along a laser beam travel path, the scanner head focusing and directing a laser beam; a working chamber for high temperature sintering of the at least one metallic powder; an airtight chamber for maintaining an inert gas seal, the airtight chamber enclosing the working chamber; a secondary powder container; a scraper for delivering the at least one metallic powder to a target area; a heating system for heating the apparatus to a setting temperature; a cylinder and piston assembly for dispensing and building the at least one metallic powder to form the metallic part; and means for controlling the sintering apparatus.
- FIGS. 1 ( a )- 1 ( c ) show assembly views of an apparatus for producing parts according to a preferred embodiment of the invention
- FIG. 2 shows a perspective exploded view of a heating system according to an embodiment of the present invention
- FIGS. 3 ( a )- 3 ( c ) show multiple views of a heating box for inert gas going through and into a working chamber according to an embodiment of the present invention
- FIGS. 4 ( a )- 4 ( c ) show detailed views of a working chamber and an air-tight chamber according to an embodiment of the present invention
- FIGS. 5 ( a )- 5 ( d ) show detailed views of the assembly of a feeding system and a dispensing mechanism for secondary powder according to an embodiment of the present invention
- FIGS. 6 ( a )- 6 ( c ) show detailed views of a piston assembly according to an embodiment of the present invention.
- FIGS. 7 ( a )- 7 ( b ) show the specially designed motion system which drives a piston moving up and down within a cylinder according to an embodiment of the present invention.
- FIGS. 1 ( a )- 1 ( c ) show assembly views of an apparatus for producing parts according to a preferred embodiment of the invention.
- FIG. 2 shows a perspective exploded view of a heating system according to an embodiment of the present invention.
- FIGS. 3 ( a )- 3 ( c ) show multiple views of a heating box for inert gas going through and into a working chamber according to an embodiment of the present invention.
- FIGS. 4 ( a )- 4 ( c ) show detailed views of a working chamber and an air-tight chamber according to an embodiment of the present invention.
- FIGS. 5 ( a )- 5 ( d ) show detailed views of the assembly of a feeding system and a dispensing mechanism for secondary powder according to an embodiment of the present invention.
- FIGS. 6 ( a )- 6 ( c ) show detailed views of a piston assembly according to an embodiment of the present invention.
- FIGS. 7 ( a )- 7 ( b ) show the specially designed motion system which drives a piston moving up and down within a cylinder according to an embodiment of the present invention.
- FIGS. 1 ( a )- 1 ( c ) show assembly views of an apparatus for producing parts according to a preferred embodiment of the invention. An apparatus for producing 3-D parts will be described in further detail hereinafter.
- FIG. 1 ( a ) is a frontal view of the apparatus
- FIG. 1 ( b ) is a side view
- FIG. 1 ( c ) is a top view of the apparatus for producing parts.
- the system of FIGS. 1 ( a )- 1 ( c ) is illustrated in exploded fashion, without cover plates and the like.
- the apparatus includes a laser 1 , a scanner head 2 , a working chamber 3 , air-tight chambers 4 a and 4 b, a secondary powder container 5 , a scraper 6 , a radiant heating plate 7 , a dispensing cylinder 10 a, a building cylinder 10 b, and a personal computer 15 .
- the laser 1 is shown somewhat schematically in FIG. 1.
- a CO 2 laser is used which can operate in a continuous mode with approximately two hundred watts maximum outlet power.
- the laser beam output of the laser 1 has a wavelength of approximately 10590 nm, which is infrared.
- the laser 1 can be modulated on or off to selectively produce a laser beam.
- the output power can also be modulated with a selectable range of 0 to 200 watt.
- the laser on or off and power output modulation are controlled by the personal computer 15 .
- the laser can be selectively controlled via the computer 15 and in accordance with a CAD file containing detailed dimensions of the desired part and its associated cross-sections.
- the scanner head 2 is mounted along the path of travel of the laser beam to focus and redirect the laser beam.
- the scanner head 2 includes a pair of mirrors driven by respective galvanometers.
- the computer 15 controls the galvanometers through a controller card.
- the controller card permits communication between the computer 15 and mirrors.
- working chamber 3 is a place where preheating, powder dispensing and sintering processes take place.
- the internal surface of the chamber 3 is made of stainless steel.
- the external surface of the chamber 3 is covered by thermal insulation material (mica, 20 mm thickness).
- thermal insulation material mica, 20 mm thickness.
- a round opening allows the laser beam to pass therethrough and to scan on the target area 8 b.
- Chamber 4 is airtight, and inert gas is enclosed in it. Inert gas is put into the chamber 4 through inlet 23 , and the air is purged out from the outlet 24 .
- a special optical crystal, which prevents the lens of scanner head 2 from contamination, is mounted on the top of the chamber 4 . The laser beam can go through the crystal with ignored energy loss.
- the container 5 is for storing secondary powder. There is a shutter pot on the bottom of the container 5 . A worm pole is inserted into the container 5 to mix the powder in the container 5 so as to be easily released. Step motor 20 drives the container 5 moving back and forth in the working chamber 3 . The scraper 6 is mounted on the container 5 . When the motor 20 drives the container 5 , the scraper 6 can move back and forth to deliver the powder to target area 8 b and level the powder surface.
- the radiant heating plate 7 is placed above leveling surface 29 .
- the radiant heating plate 7 can be driven by gas cylinder 12 to move up and down.
- the heating plate is located at the lower position so that the powder in dispensing cylinder 10 a and building cylinder 10 b can be heated effectively.
- the heating plate 7 is pushed to the upper position by cylinder 12 so that the built part can be taken out easily.
- Cylinders 10 a and 10 b house powder piston assemblies 8 a and 8 b.
- Servo motors 13 a and 13 b drive a ball screw unit (collectively, 9 a and 9 b ) through a pair of gears 11 a and 11 b. Applying the ball screw unit ( 9 a and 9 b ), rotation is converted to linear motion, and a screw shaft 9 a drives the piston assemblies 8 a and 8 b moving up and down in the cylinders 10 a and 10 b.
- a fundamental concept of the present invention is the build up of a metal part directly in a layer-by-layer manner. That is, a STL file of a part is sliced into discrete layers having a certain thickness, which cumulatively comprise the three-dimensional configuration of the part. Each layer includes a two-dimensional cross-sectional contour of the part.
- FIGS. 1 ( a )- 1 ( c ) In operation, as shown in FIGS. 1 ( a )- 1 ( c ), as the piston unit 8 a moves to the lower position, the cylinder 10 a and container 5 are filled up with different powders. Doors 16 and 17 are closed. Heating components 7 , 33 , 36 and 37 (see FIG. 2) start working to heat the working chamber 3 and powders in the cylinder 10 a and container 5 up to the setting temperature. Inert gas is conducted into the heating box through an inert gas inlet IG I and into the chamber 4 after preheating from the heating box 33 (see FIG. 2) through an inert gas outlet IG O .
- Dispensing piston 8 a moves upward by a certain distance, and a first portion of powder is lifted higher than the leveling surface 29 .
- the target piston 8 b moves downward with a certain distance so as to house the powder that will be delivered.
- the scraper 6 driven by step motor 20 sweeps from a left side of the apparatus to a right side and spreads the first portion of powder on the target area 8 b.
- the personal computer 15 controls the laser beam to selectively scan only the deposited powder within the confines of the defined boundaries. With the help of heating components, the laser beam heats the powder so as to melt, and the powder is joined together. The first sintered layer is then finished.
- the secondary powder container 5 moves to the middle position between the dispensing cylinder 8 a and target cylinder 8 b (the current position shown in FIG. 1) and stops.
- Gas cylinder 18 drives the shutter 21 on the outlet of the container 5 open, and motor 19 drives the rotating worm shaft 25 .
- the secondary powder in the container 5 is released and drops on the leveling surface 29 .
- the gas cylinder 18 drives the shutter 21 closed.
- the scraper 6 is fixed on the container 5 .
- the step motor 20 moves the container 5
- the scraper 6 moves with the container 5 together and sweeps over the leveling surface 29 .
- the secondary powder released from the container 5 is spread onto the target area 8 b.
- the laser beam selectively melts the powder according to the cross-section of the desired part.
- the target piston 8 b moves downward by an amount corresponding to the thickness of the next layer, and awaits the deposition of the next layer of powder from scraper 6 .
- FIG. 2 shows a perspective exploded view of a heating system according to an embodiment of the present invention.
- the heating system shown provides preheating for metal powder and ensures the temperature of the metal powder reaches to 400° C. prior to sintering.
- FIG. 2 schematically illustrates the preferred heating system of the present invention. The objective of the presented apparatus is melting metal powder directly.
- a preferred alternative uniquely applicable to the present invention is the application of subsidiary heating components to heat the powder to a certain temperature prior to sintering. When laser energy is added, the powder can be heated up to the melting point.
- the powder is expected to heat up to a temperature of 400° C.
- a 3000W radiant heating plate 7 is maintained in a hanging position over the leveling surface 29 to achieve the predetermined temperature.
- the heating plate 7 drops down by weight, and two stoppers 38 fixed on the wall of the working chamber 3 support the heating plate 7 .
- the powder in cylinder 10 a and 10 b can absorb heat radiated by the heating plate 7 .
- gas cylinders 12 shown in FIG. 1) controlled by computer 15 push the heating plate 7 upwardly so that the produced part can be removed easily.
- Opening 34 on the heating plate 7 is meant for permitting the laser beam to pass through.
- strip heaters 37 are installed under the platform 8 a and 8 b to ensure the powder in the cylinders is heated to the required temperature.
- Secondary powder in the container 5 absorbs heat in at least two ways.
- the radiant heating plate 7 radiates heat to the powder in the container 5 .
- strip beaters 35 and 36 are installed on two sides of the container 5 to ensure the powder in container 5 is heated to the required temperature.
- Inert gas such as nitrogen
- Inert gas may be very cold when it is just released from the gas cylinder. If a cold gas is conducted into the working chamber 3 , it could undesirably effect the temperature in the chamber 3 . Therefore, the heating box 33 preheats the inert gas prior to the gas entering the chamber 3 (as shown in FIG. 2 ).
- FIGS. 3 ( a )- 3 ( c ) show multiple views of a heating box 33 for preheating inert gas prior to the inert gas entering a working chamber according to an embodiment of the present invention.
- FIG. 3 ( a ) is a top view
- FIG. 3 ( b ) is a frontal view
- FIG. 3 ( c ) is a side view of the heating box 33 according to a preferred embodiment.
- the heating box 33 includes two boxes, an inner airtight box 43 for heating inert gas and an outer box 44 for thermal insulation.
- In the inner box 43 there are three 350W heaters 39 installed.
- a thermal coupler 41 is placed into the box 43 for closed-loop temperature control. The air between the inner box 43 and the outer box 44 prevents the heat in the box 43 from scattering.
- Inert gas used for oxidation prevention enters the heating box 43 from the entrance 40 .
- the inert gas is heated as it passes through the heater 39 and is then released from the exit 42 .
- the exit 42 is connected with the working chamber 3 at the junction 23 (shown in FIG. 2) from which the preheated inert gas IG O enters into the working chamber 3 .
- the powder in chamber 3 can reach the desired temperature of 400° C. when the foregoing components are used as described hereinabove.
- FIGS. 4 ( a )- 4 ( c ) show detailed views of a working chamber and an air-tight chamber according to an embodiment of the present invention.
- FIG. 4 ( a ) is a cross-sectional frontal view
- FIG. 4 ( b ) is a top view
- FIG. 4 ( c ) is a side view of the two chambers.
- the working chamber and the airtight chamber help to maintain the temperature of the metal powder at the desired temperature/set point.
- the structure of the working chamber 3 and the airtight chamber 4 will now be described in further detail.
- An inner part of the working chamber 3 is a stainless steel cover. There is a door 16 in front, and an opening 22 on the top of the chamber 3 for permitting the laser beam to enter. On the back wall of the chamber 3 , there is an inlet 23 for the entrance of inert gas and an outlet 24 the exhaust of inert gas.
- a thermal insulation material 45 e.g., mica and/or its equivalent, having a thickness of approximately 20 mm, covers the exterior of the chamber 3 .
- a working plate 29 forms the floor of the chamber 3 and a thermal insulation plate 30 is backed up beneath the working plate 29 .
- Four thermal insulation bars 47 are put under the insulation plate 30 , and a space with 20 mm thickness is therefore left between the insulation plate 30 and base plate 31 for further thermal insulation.
- the airtight chamber 4 surrounds the working chamber 3 .
- the chamber 4 is also made of stainless steel sheet, and is fixed on the base plate 31 .
- the chamber 4 is formed of two parts 4 a and 4 b. Part 4 a surrounds the working chamber 3 , and part 4 b covers the motion system of the scraper 6 and the secondary container 5 . Air can flow between part 4 a and part 4 b.
- a window 22 is mounted on the top of the chamber 4 for permitting the CO 2 laser to pass through while still preventing gas within the chamber 4 from leakage. Inert gas is sealed in the chamber 4 . A space is left between chamber 3 and chamber 4 that helps to achieve good thermal insulation effect.
- FIGS. 5 ( a )- 5 ( d ) show detailed views of the assembly of a feeding system and a dispensing mechanism for secondary powder according to an embodiment of the present invention.
- FIG. 5 ( a ) is a top view
- FIG. 5 ( b ) is a partial, cross-sectional frontal view
- FIG. 5 ( c ) is a left side view
- FIG. 5 ( d ) is a right side view of the assembly of the feeding system and the dispensing mechanism.
- the secondary powder container 5 is open on the top.
- the powder can be added into the container 5 and absorb heat from the heating plate 7 .
- the scraper 6 is fixed on one side 77 of the container 5 .
- On the bottom of the container there is a slot left for powder releasing.
- a worm shaft 25 inserts into the container 5 and can be rotated by the motor 19 .
- the stirring action will help fine powder to release smoothly.
- a shutter 21 fixed on a shaft 26 driven by the gas cylinder 18 , normally closes the slot. When the gas cylinder 18 is inflated, the shaft 26 is driven to rotate, and the shutter 21 installed on the shaft 26 will open.
- the two side-walls 75 and 76 of the container 5 are connected with plates 79 and 80 respectively through thermal insulation plates 77 and 78 so as to avoid heat conduction to the motion parts.
- the plates 79 and 80 are fixed on moving platform 84 which is connected to belt 82 .
- the belt 82 is twined on a pair of belt wheels 83 and 86 and the belt wheel 83 is connected with the step motor 20 .
- the rotary action of the motor 20 is converted to the linear motion of the belt 82 .
- the motion of the belt 82 drives the container 5 and scraper 6 back and forth together with the moving platform 84 .
- the motion of the moving platform 84 is guided by a pair of guide rails 85 .
- the motion system including components 19 , 20 , 82 , 83 , 85 and 86 installed on part 4 b, should avoid working in a high temperature environment to guarantee the motion accuracy and increase the lifetime of precision components.
- Air can flow from part 4 a to part 4 b through slot 73 . Since the working area 4 a is at a high temperature, the slot 73 should be opened as small as possible.
- a flexible thermal insulation belt 74 is connected with the container 5 . The flexible thermal insulation belt 74 can move together with the container 5 and seals the slot 73 so as to prevent heat in area 4 a from being transferred into area 4 b through radiation and convection.
- FIGS. 6 ( a )- 6 ( c ) show detailed views of a piston assembly according to an embodiment of the present invention.
- the 3D objective is built on the piston assembly and the unsintered powder is stored therein.
- FIG. 6 ( a ) is a partial cross-sectional view
- FIG. 6 ( b ) is a second partial cross-sectional view
- FIG. 6 ( c ) is an enlarged view of a portion of FIG. 6 ( b ) of the piston assembly according to an embodiment of the present invention.
- FIG. 6 illustrates the structure of piston 8 a and cylinder 10 a.
- the temperature of the powder loaded in the cylinder 10 a is about 400° C.
- Commonly used sealant, such as rubber or blanket, cannot withstand such a high temperature.
- the rigid seal requires the piston 8 a and cylinder 10 a to be precision machined, and the tolerance must be tightly controlled.
- piston 8 a needs to move in the cylinder 10 a, the alignment between the piston, cylinder and precise motion system is very difficult with the rigid seal.
- the different thermal expansion of the cylinder 10 a and the piston 8 a may jam the motion of the piston.
- piston rings 50 are used for maintaining a seal.
- the piston rings 50 are made from cast iron.
- the piston rings 50 can work properly in 800° C. temperature.
- cast iron possesses good sand bearing, e.g. it is advantageous for use with seal powder material.
- the diameter of the piston ring is approximately 252 mm in a preferred embodiment.
- the existence of an oblique gap 59 in the piston ring and the elasticity of the material make the diameter of the piston ring adjustable.
- the diameter of the cylinder 10 a, in which piston unit moves up and down, is approximately 250 mm in a preferred embodiment.
- FIGS. 7 ( a )- 7 ( b ) show a specially designed motion system which drives a piston moving up and down within a cylinder according to an embodiment of the present invention.
- FIG. 7 ( a ) is a side and top view and
- FIG. 7 ( b ) is an opposite side and partial top view of the motion system.
- the motion system of the piston unit will be described in greater detail hereinafter with specific reference to FIGS. 7 ( a )- 7 ( b ).
- a ball screw unit 9 , guide pin 28 a and bush 28 b connect piston unit 8 a and motion system together.
- a ball screw nut 9 b and a screw shaft 9 a are applied here to precisely transfer a rotary action to linear motion.
- Servo motor 13 a drives the ball screw nut 9 b turning through a pair of precise gears 11 a and 11 b. Due to binding by component 62 in the vertical direction, the ball screw nut 9 b only rotates without movement in this direction. Due to the rotating action, the screw nut 9 b precisely drives the screw shaft 9 a moving in the vertical direction.
- the linear motion of the piston unit is guided and supported by guide pin 28 a and guide bush 28 b, and the rolling match between the guide pin 28 a and guide bush 28 b makes the motion of piston steady and easy.
Abstract
Description
Claims (10)
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US09/993,720 US6621039B2 (en) | 2000-11-27 | 2001-11-27 | Method and apparatus for creating a free-form three-dimensional metal part using high-temperature direct laser melting |
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US25319800P | 2000-11-27 | 2000-11-27 | |
US09/993,720 US6621039B2 (en) | 2000-11-27 | 2001-11-27 | Method and apparatus for creating a free-form three-dimensional metal part using high-temperature direct laser melting |
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US6621039B2 true US6621039B2 (en) | 2003-09-16 |
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US09/993,720 Expired - Fee Related US6621039B2 (en) | 2000-11-27 | 2001-11-27 | Method and apparatus for creating a free-form three-dimensional metal part using high-temperature direct laser melting |
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US (1) | US6621039B2 (en) |
EP (1) | EP1347853B1 (en) |
CN (1) | CN1476362A (en) |
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Also Published As
Publication number | Publication date |
---|---|
DE60114453D1 (en) | 2005-12-01 |
DE60114453T2 (en) | 2006-07-13 |
EP1347853B1 (en) | 2005-10-26 |
EP1347853A1 (en) | 2003-10-01 |
US20020090313A1 (en) | 2002-07-11 |
AU2002222885A1 (en) | 2002-06-03 |
WO2002042023A1 (en) | 2002-05-30 |
CN1476362A (en) | 2004-02-18 |
EP1347853A4 (en) | 2004-07-21 |
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